[ CAS No. 281678-66-8 ] {[proInfo.proName]}

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Quality Control of [ 281678-66-8 ]

COA NMR CNMR HPLC LC-MS

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SDS Specification

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Product Details of [ 281678-66-8 ]

CAS No. :	281678-66-8	MDL No. :	MFCD07644612
Formula :	C₈H₇Br₂ClO	Boiling Point :	-
Linear Structure Formula :	-	InChI Key :	-
M.W :	314.40	Pubchem ID :	-
Synonyms :

Safety of [ 281678-66-8 ]

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Application In Synthesis of [ 281678-66-8 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

Upstream synthesis route of [ 281678-66-8 ]
Downstream synthetic route of [ 281678-66-8 ]

[ 281678-66-8 ] Synthesis Path-Upstream 1~1

1
[ 68-12-2 ]
[ 281678-66-8 ]
[ 196799-45-8 ]

Yield	Reaction Conditions	Operation in experiment
100%	Stage #1: With n-butyllithium In tetrahydrofuran; hexane at -40℃; for 0.25 h; Stage #2: at -40℃; for 1.5 h;	A solution of n-butyl lithium (1.54M-n-hexane solution, 29.2ml, 44.97mmol) in THF (40ml) was added with a solution of Step 1 compound (4.75g, 15.00mmol) in THF (20ml) at -40°C and stirred for 15 minutes. Next, DMF (2.19g, 44.97mmol) was added and the mixture was stirred at -40°C for 1.5 hours. The reaction was stopped by adding water, and the reaction solution was concentrated. Liquid separation was carried out with ethyl acetate-water, the organic layer was washed with 1M-hydrochloric acid and saturated sodium chloride water, dried with anhydrous sodium sulfate, and concentrated to obtain the title compound (2.32g, quant) as a colorless crystal. ¹H-NMR (300MHz, CDCl₃) δ=3.25 (2H, t, J=7.2Hz), 4.74 (2H, t, J=7.2Hz), 6.93 (1H, t, J=7.5Hz), 7.41 (2H, d, J=7.5Hz), 7.58 (1H, d, J=7.5Hz), 10.20 (1H, s).

Reference： [1] Patent: EP1878734, 2008, A1, . Location in patent: Page/Page column 15
[2] Advanced Synthesis and Catalysis, 2007, vol. 349, # 1-2, p. 193 - 203
[3] Tetrahedron Letters, 2000, vol. 41, # 14, p. 2269 - 2273

[ 281678-66-8 ] Synthesis Path-Downstream 1~3

1
[ 3570-58-9 ]
[ 608-33-3 ]
[ 281678-66-8 ]

Reference： [1]Tetrahedron Letters,2000,vol. 41,p. 2269 - 2273

2
[ 68-12-2 ]
[ 281678-66-8 ]
[ 196799-45-8 ]

Yield	Reaction Conditions	Operation in experiment
100%		A solution of n-butyl lithium (1.54M-n-hexane solution, 29.2ml, 44.97mmol) in THF (40ml) was added with a solution of Step 1 compound (4.75g, 15.00mmol) in THF (20ml) at -40C and stirred for 15 minutes. Next, DMF (2.19g, 44.97mmol) was added and the mixture was stirred at -40C for 1.5 hours. The reaction was stopped by adding water, and the reaction solution was concentrated. Liquid separation was carried out with ethyl acetate-water, the organic layer was washed with 1M-hydrochloric acid and saturated sodium chloride water, dried with anhydrous sodium sulfate, and concentrated to obtain the title compound (2.32g, quant) as a colorless crystal. 1H-NMR (300MHz, CDCl3) delta=3.25 (2H, t, J=7.2Hz), 4.74 (2H, t, J=7.2Hz), 6.93 (1H, t, J=7.5Hz), 7.41 (2H, d, J=7.5Hz), 7.58 (1H, d, J=7.5Hz), 10.20 (1H, s).

Reference： [1]Patent: EP1878734,2008,A1 .Location in patent: Page/Page column 15
[2]Advanced Synthesis and Catalysis,2007,vol. 349,p. 193 - 203
[3]Tetrahedron Letters,2000,vol. 41,p. 2269 - 2273

3
[ 608-33-3 ]
[ 107-04-0 ]
[ 281678-66-8 ]

Yield	Reaction Conditions	Operation in experiment
100%	With potassium carbonate; In N,N-dimethyl-formamide; at 20℃; for 16h;	A solution comprising <strong>[608-33-3]2,6-dibromophenol</strong> (3.90g, 15.00mmol), potassium carbonate (2.48g, 17.94mmol) and DMF (40nl) was added with 1-bromo-2-chloro ethane (4.30g, 29.98mmol) and stirred at room temperature for 16 hours. The reaction solution was concentrated and liquid separation was carried out with ethyl acetate-water. The organic layer was washed with saturated sodium chloride water and dried with anhydrous sodium sulfate. The residue obtained by concentration was purified by silica gel column chromatography (n-hexane) to obtain the target compound (4.75g, quant.) as a colorless oily substance. 1H-NMR (300MHz, CDCl3) delta=3.91 (2H, t, J=6.6Hz), 4.27 (2H, t, J=6.6Hz), 6.89 (1H, t, J=7.8Hz), 7.51 (2H, d, J=7.8Hz).

Reference： [1]Patent: EP1878734,2008,A1 .Location in patent: Page/Page column 14-15
[2]Advanced Synthesis and Catalysis,2007,vol. 349,p. 193 - 203

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Precautionary Statements-General
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P304 + P312	IF INHALED: Call a POISON CENTER or doctor/physician if you feel unwell.
P304 + P340	IF INHALED: Remove victim to fresh air and Keep at rest in a position comfortable for breathing.
P304 + P341	IF INHALED: If breathing is difficult, remove victim to fresh air and keep at rest in a position comfortable for breathing.
P305 + P351 + P338	IF IN EYES: Rinse cautiously with water for several minutes. Remove contact lenses, if present and easy to do. Continue rinsing.
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P332 + P313	IF SKIN irritation occurs: Get medical advice/attention.
P333 + P313	IF SKIN irritation or rash occurs: Get medical advice/attention.
P335 + P334	Brush off loose particles from skin. Immerse in cool water/wrap in wet bandages.
P337 + P313	IF eye irritation persists: Get medical advice/attention.
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H200	Unstable explosive
H201	Explosive; mass explosion hazard
H202	Explosive; severe projection hazard
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H240	Heating may cause an explosion
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H401	Toxic to aquatic life
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H411	Toxic to aquatic life with long-lasting effects
H412	Harmful to aquatic life with long-lasting effects
H413	May cause long-lasting harmful effects to aquatic life
H420	Harms public health and the environment by destroying ozone in the upper atmosphere

[ CAS No. 281678-66-8 ] {[proInfo.proName]}

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[ 281678-66-8 ] Synthesis Path-Upstream 1~1

[ 281678-66-8 ] Synthesis Path-Downstream 1~3

Precautionary Statements-General

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